Potassium Carbonate → HCID 178451986, 화합물

HRID 1408339

반응식

HRID 1408339 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]#[N:15])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C([O-])([O-])=O.[K+].[K+].Cl.[NH2:23][OH:24]>O.CCO>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14](=[NH:15])[NH:23][OH:24])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 1514443Tert-butyl 4-cyanopiperidine-1-carboxylate

생성물 1

HCID 178451986HCID 178451986, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a mixture of 4-cyano-piperidine-1-carboxylic acid tert-butyl ester (6.3 g, 30 mmol), K2CO3 (4.2 g, 30 mmol) in H2O (50 mL) and EtOH (30 mL) was added hydroxylamine hydrogenchloride (4.17 g, 60 mmol). The mixture was heated under reflux overnight, cooled to room temperature and ethanol was removed in vacuo. The residue was extracted with EtOAc (300 mL). The organic layer was washed successively with H2O and brine. After drying (Na2SO4), the solvent was removed to afford the desired product.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux overnight
  3. customethanol was removed in vacuo
  4. extractionThe residue was extracted with EtOAc (300 mL)
  5. washThe organic layer was washed successively with H2O and brine
  6. dry with materialAfter drying (Na2SO4)
  7. customthe solvent was removed

출처 및 근거

ORD 기록
ord-e536042bad33491cb5cec88fb0db431a
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08921350B2

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